[关键词]
[摘要]
目的 利用原子转移自由基聚合(ATRP)技术制备姜黄素分子印迹复合膜(MIM),并建立一种实际样品中姜黄素分离富集的方法。方法 以姜黄素为模板分子,甲基丙烯酸为功能单体,氯化亚铜为催化剂,五甲基二乙烯三胺为配体,聚偏氟乙烯微孔滤膜为基膜,采用热聚合法制备姜黄素MIM;通过扫描电镜(SEM)考察了MIM的微观结构;采用静态和动态吸附实验对MIM的最大吸附量和吸附平衡时间进行考察,并对选择性渗透能力进行研究;以MIM为渗透装置中的膜材料,结合HPLC法对样品中的姜黄素进行分离、富集、检测。结果 制备的MIM孔穴分布规则且大小均匀;最大吸附量达3.81 mg/g,且15 min即可达到吸附平衡;在阿魏酸、槲皮素和姜黄素的选择性渗透过程中,MIM对姜黄素具有较高的选择渗透能力;对生姜、姜黄、咖喱中的姜黄素进行加标回收试验,其平均回收率分别为(94.100±3.952)%、(98.300±3.637)%、(97.900±3.133)%,RSD均小于4.2%,检出限为1.76 μg/kg。结论 制备的姜黄素MIM吸附速度快、选择性强,为姜黄素的分离、富集提供一种新的材料,同时也为其他中药化学成分的研究提供借鉴。
[Key word]
[Abstract]
Objective To prepare the molecularly imprinted composite membrane of curcumin by the atom transfer radical polymerization (ATRP) technique and develop a method for the separation and enrichment of curcumin in actual samples. Methods Curcumin MIM were prepared by thermal polymerization method using curcumin as template molecule, methylacrylic acid as functional monmers, cuprous chloride as catalyst, pentamethyldiethylenetriamine as ligand, and polyvinylidene fluoride as base membrane. The microstructure of MIM was investigated by SEM. The maximum adsorption and adsorption equilibrium time of MIM were investigated by static and dynamic adsorption experiment, and the selective penetration capacity was studied. The MIM as membrane material of osmotic device combined with HPLC was used for separation, enrichment and determination of curcumin in samples. Results The results showed that the prepared curcumin MIM had a regular distribution of pores and a uniform size. The maximum adsorption capacity was 3.81 mg/g, and the adsorption equilibrium could be achieved in 15 min. In the selective permeation process of ferulic acid, quercetin and curcumin, MIM had a high selective permeability to curcumin. The average recovery rates of curcumin in ginger, turmeric and curry were (94.100 ±3.952)%, (98.300 ±3.637)%, and (97.900 ±3.133)%, respectively. The RSD was less than 4.2%. The limit of detection was 1.76 μg/kg. Conclusion The prepared MIM is a new material for strong selectivity, separation and enrichment of Chinese medicine curcumin with fast adsorption speed. At the same time, it also provides reference for chemical composition research of other Chinese materia medica.
[中图分类号]
R283.6
[基金项目]
黑龙江省自然科学基金资助项目(QC2018073);黑龙江省教育厅科研项目(135109201);黑龙江省教育厅科研项目(135209224);齐齐哈尔大学研究生创新项目(YJSCX2018-016X);齐齐哈尔大学研究生创新项目(YJSCX2017-020X)